Investigating the Effects of Operating Parameters of a … · · 2017-07-22of reflux ratio and reboiler duty separately affects the operation of the reaction integrated distillation

International Journal of Science and Research (IJSR) ISSN (Online): 2319-7064

Index Copernicus Value (2013): 6.14 | Impact Factor (2013): 4.438

Volume 4 Issue 7, July 2015

www.ijsr.net Licensed Under Creative Commons Attribution CC BY

Investigating the Effects of Operating Parameters of

a Reaction Integrated Distillation Process for SAME

Production Using Aspen PLUS

Abdulwahab GIWA1, Saidat Olanipekun GIWA

2

1Chemical and Petroleum Engineering Department, College of Engineering, Afe Babalola University, KM. 8.5, Afe Babalola Way, 360231,

Ado-Ekiti, Ekiti State, Nigeria

2Chemical Engineering Department, Faculty of Engineering and Engineering Technology, Abubakar Tafawa Balewa University,

Tafawa Balewa Way, 740004, Bauchi, Bauchi State, Nigeria

Abstract: The effects of some operating parameters of a reaction integrated distillation process used for the production of a biodiesel

type have been studied in this research work. The operating parameters considered were reflux ratio and reboiler duty while the

biodiesel type produced was stearic acid methyl ester (SAME) that was obtained from the esterification reaction between stearic acid

and methanol. The production of the biodiesel was accomplished theoretically with the aid of a process simulator known as Aspen

PLUS using RadFrac column that had 32 stages including the condenser and the reboiler and that was divided into three (rectifying,

reaction and stripping) sections, excluding the condenser and the reboiler. The reaction was taken to occur in the middle, which was the

reaction section of the column as well as in the reboiler. In order to study the effects of the operating parameters, both simulation and

sensitivity analysis of the process were carried out using the process simulator. Based on the observations of the simulation and the

sensitivity analysis, optimization was carried out also using Aspen PLUS. The results obtained revealed that separate variations of

reflux ratio, from 1 to 10, and reboiler duty, from 0.1 to 1 kW, while keeping other simulation parameters constant yielded a bottom

product with very high purity SAME at a reflux ratio of 1 and a reboiler duty of 0.1 kW. However, the combination of these values of

the operating parameters could not converge when used to run the developed model of the process. Furthermore, using the optimum

values of the reflux ratio and the reboiler duty that were estimated to be 2.23 and 0.90 kW, respectively to run the developed process

model, SAME mole fraction of 0.9993 was obtained from the bottom product of the column. Therefore, it has been discovered that each

of reflux ratio and reboiler duty separately affects the operation of the reaction integrated distillation process, but considering their

combined effects simultaneously and optimizing are very necessary in order to achieve very high purity of the desired product.

Keywords: Stearic acid methyl ester (SAME), modelling and simulation, sensitivity analysis, optimization, Aspen PLUS.

1. Introduction

Biodiesel, as an alternative fuel, is currently receiving

attentions both in academics and in industries owing to the

limited availability of conventional petroleum diesel as well

as environmental concerns. This fuel can be directly used to

replace petroleum diesel without modifying diesel engines

since their properties such as specific gravity, cetane number,

viscosity, cloud point, and flash point, are similar

(Simasatitkul et al., 2011; Giwa et al., 2014; Giwa et al.,

2015). It is a very good promising alternative to conventional

petroleum based diesel fuel. Among its important advantages

are that it can be derived from a renewable domestic resource

(e.g., waste cooking oil), it reduces carbon dioxide emissions

by about 78%, and it is nontoxic and biodegradable. All these

benefits have made biodiesel a very good environmental

friendly fuel (Wang et al., 2004; Jaya and Ethirajulu, 2011;

Giwa et al., 2014; Giwa et al., 2015).

According to Giwa et al. (2014), biodiesel with high purity

can be produced via esterification reaction of fatty acids with

alcohols (methanol or ethanol). Also, Omota et al., (2003)

proposed the use of batch reactor for the esterification of

fatty acid and alcohol into fatty acid methyl ester (biodiesel).

However, the production of biodiesel from the esterification

reaction in the conventional batch reactor has been found to

possess many problems due to low conversion, heavy capital

investments and high energy costs (Gao et al., 2007). In an

attempt to resolve these problems, an advanced technology

known as “reaction integrated distillation” has been

developed (Kusmiyati and Sugiharto, 2010; Giwa et al.,

2014; Giwa et al., 2015).

Reaction integrated distillation is a process that combines

separation and chemical reaction in a single unit. It is very

attractive whenever conversion is limited by reaction

equilibrium (Balasubramhanya and Doyle III, 2000; Lai et

al., 2007; Giwa and Karacan, 2012e; Giwa and Giwa, 2012;

Giwa, 2013). It is sometimes an excellent alternative to

conventional flowsheets with different reaction and

separation sections (Al-Arfaj and Luyben, 2002; Giwa and

Karacan, 2012d). It combines the benefits of equilibrium

reaction with distillation to enhance conversion (Giwa and

Karacan, 2012a; Giwa and Karacan, 2012c). As in this

process, combining reaction and distillation has several

advantages that include: a) shift of chemical equilibrium and

an increase of reaction conversion by simultaneous reaction

and separation of products, b) suppression of side reactions

and c) utilization of heat of reaction for mass transfer

operation (Giwa and Karacan, 2012b). The utilization of heat

of reaction for mass transfer operation, which resulted into

low external energy consumption of the process, actually,

give rise to reduced investment and operating costs (Giwa,

2012).

Paper ID: SUB157055 2349





Although this (reaction integrated distillation) process for

biodiesel production is associated with many benefits, the

integration of both chemical reaction and separation in a

single unit has made its behaviour complex especially when

high boiling materials such as fatty acids are involved. As

such, there is a need to handle this process, first, using

process simulators like ChemCAD, Aspen HYSYS, Aspen

PLUS, and so on so as to gain ideas into how it will perform

in real life and provide necessary measures to handle any

unusual circumstance.

Based on this, Karacan and Karacan (2014) applied Aspen

HYSYS to simulate a reactive distillation process for a fatty

acid methyl ester production. In the work, canola oil and

methanol were used as feedstocks while potassium hydroxide

and potassium methoxide were used as catalysts. Also,

Simasatitkul et al. (2011) carried out the simulation of a

reactive distillation process for a fatty acid methyl ester

production from transesterification of soybean oil and

methanol, catalyzed by sodium hydroxide, and it was

concluded from their work that methanol and soybean oil

should be fed into the column at the first stage. Furthermore,

Samakpong et al. (2012) simulated and optimized a fatty acid

methyl ester production using reactive distillation of rubber

seed oil, and they discovered that feedstock with high free

fatty acids (FFAs) could not undergo transesterification with

alkaline catalyst. However, they discovered that the

esterification of palmitic acid and methanol to biodiesel

could be achieved via reactive distillation with 100%

conversion and without feeding excess methanol. They also

found that reactive distillation made hydrolysis (reverse of

esterification) reaction to be negligible because water was

constantly removed from the process. Giwa et al. (2014)

investigated the performances of some fatty acids used for

the production of fatty acid methyl esters in a reactive

distillation column with the aid of Aspen HYSYS. The fatty

acids considered were oleic acid, which was discovered,

according to Kusmiyati and Sugiharto (2010), to give fatty

acid methyl ester that had the quality required to be a diesel

substitute, and some other ones (stearic acid, linoleic acid

and palmitic acid) found to be present in jatropha oil.

Methanol was used as the alcohol for the reaction. The

results they obtained revealed that palmitic acid had the best

performance in fatty acid methyl ester production.

Nwambuonwo et al. (2015) modelled, simulated and

optimized a reactive distillation process used for the

production of fatty acid methyl ester (FAME) by considering

an esterification reaction between palmitic acid and methanol

to give methyl palmitate (FAME) and water (by-product)

with the aid of Aspen HYSYS, and they were able to develop

a model that could represent the process very well based on

the result of the validation that was done. Santander et al.

(2010) used response surface methodology and Aspen PLUS

process simulator to investigate biodiesel production in a

reactive distillation using castor oil.

As can be noticed, researches already carried out on the

application of Aspen PLUS for biodiesel production are few.

Therefore, this work has been carried out to apply Aspen

PLUS to a reaction integrated (reactive) distillation process

used for SAME (stearic acid methyl ester) production in

order to study the effects of reflux ratio and reboiler duty on

the purity of the SAME product given by the process. In

addition, the optimum values of the operating parameters

(reflux ratio and reboiler duty) that could give very high

purity of the desired product were estimated, also, with the

aid of Aspen PLUS.

2. Methodology

The developed model of the Aspen PLUS (Aspen, 2012)

reaction integrated distillation process used, in this work, for

the production of SAME from the esterification reaction

between stearic acid and methanol (given in Equation 1) is

shown in Figure 1. The model comprised two (upper and

lower) feed streams. The fatty acid used, which was stearic

acid, was passed from the upper feed stream because it was

less volatile than the alcohol (methanol) used that was fed

through the lower feed stream of the column. Both feeds

were introduced into the reaction integrated distillation

column at room temperature and pressure. The details of the

data used for the development and the simulation of the

model are given in Table 1.

OHOHCOHCHOHC 223819323618 (1)

After the model was developed and simulated using the data

given in Table 1, the effects of reflux ratio and reboiler duty

on the mole fractions of the components (unreacted stearic

acid, unreacted methanol, produced biodiesel and water

given as by-product) obtained from the bottom product

stream of the column were studied by utilizing the sensitivity

analysis section of Model Analysis Tool of Aspen PLUS.

Given in Table 2 are the ranges of the values used for the

sensitivity analysis.

The combined values of the operating parameters required

for the production of high purity biodiesel were later

estimated by carrying out the optimization of the process

with the aid of the optimization section of the Model

Analysis Tool of Aspen PLUS. As implied, the manipulated

variables of the optimization were the reflux ratio and the

reboiler duty while the objective function was the

maximization of the mole fraction of biodiesel (SAME)

present in the bottom product of the reaction integrated

distillation column. In addition, the lower and the upper

bounds of the manipulated variables were set to be the same

as those used for the sensitivity studies (see Table 2).






RDCOLUMN

RDBPROD

RDLFEED

RDTPRODRDUFEED

Figure 1: Aspen PLUS reaction integrated distillation column

Table 1: Aspen PLUS reaction integrated distillation process

model development parameters

Parameter Reactive Distillation Process

Stearic acid feed (Upper feed)

Flow rate (L/min) 0.03

Temperature (oC) 25

Pressure (atm) 1

Methanol feed (Lower feed)

Flow rate (L/min) 0.01

Temperature (oC) 25

Pressure (atm) 1

Property method Wilson

Reaction

Type Equilibrium

Reacting phase Liquid

Keq basis Molarity

Keq computation source Gibbs energy

Column

Type RadFrac

Total number of stages 32

Stearic acid feed stage 11

Methanol feed stage 20

Reaction section stages 11-20 and reboiler (stage 32)

Condenser (stage 1) type Total

Reboiler type Kettle

Valid phases Vapour-Liquid

Reflux ratio 3

Reboiler duty (kW) 0.7

Condenser pressure (atm) 1

Table 2: Ranges of operating parameters used for sensitivity

analysis

Parameter Lower limit Upper limit Step

Reflux ratio (kgmol/min

liquid / kgmol/min distillate) 1 10 0.5

Reboiler duty (kW) 0.1 1 0.1

3. Results and Discussion

The results obtained from the simulation of the Aspen PLUS

model developed for the production of stearic acid methyl

ester (SAME), which is a biodiesel, were as given in Figure

2. From the figure, it was seen that the reaction conversion

was very high because the mole fraction of the reactants

(stearic acid and methanol) present and remaining in the

stages of the column at the end of the simulation was very

low. Also noticed from the results was that water had the

highest mole fraction throughout the column except in the

condenser (stage 1) and the reboiler (stage 32). In the bottom

section of the column, from where the product was collected,

the component with the highest mole fraction was found to be

SAME (the desired product of the process). This observation

made at the reboiler section of the column that SAME had

the highest mole fraction there actually indicated that proper

separation of the desired product was achieved in the column.






0.00

0.10

0.20

0.30

0.40

0.50

0.60

0.70

0.80

0.90

1.00

1 3 5 7 9 11 13 15 17 19 21 23 25 27 29 31

Liq

uid

mole

fra

ctio

n

Column stage

Stearic acid

Methanol

SAME

Water

Figure 2: Liquid mole fraction profiles obtained from the simulation of the developed Aspen PLUS model

Figure 3 shows the results obtained when the effect of reflux

ratio on the purity of the product obtained from the reaction

integrated distillation process was studied. As can be

observed from the figure, as the reflux ratio was varied from

1 to 10, while keeping other variables of the model constant

at their simulation values given in Table 1, the mole fraction

of each of the components present in the bottom product was

found to change. According to the result, the highest purity of

the desired product (SAME) was achieved when the reflux

ratio was 1. At that reflux ratio of 1, the mole fraction of the

by-product of the process (water) was found to be negligible,

but, thereafter, it increased as the reflux ratio was increased.

At the reflux ratio of 5.5 and henceforth, the mole fractions

of the two products of the process (SAME and water) were

found to be the exactly the same. Also discovered from the

results given in Figure 3 was that the mole fraction of stearic

acid present in the column after the simulation with each

reflux ratio was negligible while that of methanol was also

negligible but later increased when the reflux ratio was

greater than 5.

Furthermore, the effect of reboiler duty on the composition of

the product obtained from the bottom section of the reaction

integrated distillation column was also investigated, and the

results of the investigation are given in Figure 4. It was

observed from the figure that the highest mole fraction of

SAME was obtained when the reboiler duty of the column

was 1 kW. At that value of the reboiler duty, the mole

fraction of the other product of the process (water) was very

small. As the reboiler duty was varied from 0.1 to 0.5 kW,

the mole fraction of methanol was found to decrease to

almost zero, indicating its high consumption in the process,

and it remained constant (at almost zero) thereafter up to the

maximum reboiler duty of 1 kW that was investigated while

that (the mole fraction) of stearic acid was negligible at all

the values of the reboiler duty considered. As can be seen

from the sensitivity results given in Figures 3 and 4, the

highest mole fraction of SAME was achieved at low reflux

ratio of 1 and at high reboiler duty of 1 kW considered.

However, when the values (a reflux ratio of 1 and a reboiler

duty of 1 kW) were used to run the model, it did not

converge. This was an indication that the values of each of

the operating parameters obtained, separately, that gave high

purity biodiesel (SAME) could not be used together to run

the plant and get high purity product.






0.00

0.10

0.20

0.30

0.40

0.50

0.60

0.70

0.80

0.90

1.00

1 2 3 4 5 6 7 8 9 10

Liq

uid

mole

fra

ctio

n

Reflux ratio

Stearic acid

Methanol

SAME

Water

Figure 3: Effect of reflux ratio on the composition of bottom product of the process

0.00

0.10

0.20

0.30

0.40

0.50

0.60

0.70

0.80

0.90

1.00

0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1

Liq

uid

mo

le f

ract

ion

Reboiler duty (kW)

Stearic acid

Methanol

SAME

Water

Figure 4: Effect of reboiler duty on the composition of bottom product of the process

Based on this, the interactions of the operating parameters

(reflux ratio and reboiler duty) investigated were plotted

together, as shown in Figure 5, to estimate their point of

intersection, and this point was obtained to be reflux ratio of

5 and a reboiler duty of 0.5 kW. Using these values of the

point of intersection to run the developed model of the

reaction integrated distillation process, the mole fraction of

the biodiesel (SAME) obtained was found to be 0.4062. This

value was observed not to be favourable, and, hence, it was

deemed necessary to find the best operating parameters that

would give a product having high mole fraction of SAME,

and the process optimization was, therefore, carried out with

the aid of Aspen PLUS.






0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1

0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9

1

0.00

0.10

0.20

0.30

0.40

0.50

0.60

0.70

0.80

0.90

1.00

1 2 3 4 5 6 7 8 9 10

Reboiler duty (kW)

Liq

uid

SA

ME

mole

fra

ctio

n

Liq

uid

SA

ME

mole

fra

ctio

n

Reflux ratio

Reflux ratio

Reboiler duty

Figure 5: Liquid SAME mole fraction obtained from the separate interactions of the parameters

The results obtained from the optimization carried out in

which the maximization of the mole fraction of SAME

obtained from the bottom section of the column was taken as

the objective function are given in Table 3. According to the

table, SAME (the biodiesel produced) having purity as high

as a mole fraction of 0.9993 was theoretically obtained as the

product when the optimum values of the reflux ratio and the

reboiler duty were 2.23 and 0.90 kW, respectively.

Table 3: Optimum parameters of the process Parameter Value

Reflux ratio 2.23

Reboiler duty (kW) 0.90

Objective function (Bottom SAME mole fraction) 0.9993

0.00

0.10

0.20

0.30

0.40

0.50

0.60

0.70

0.80

0.90

1.00

1 3 5 7 9 11 13 15 17 19 21 23 25 27 29 31

Liq

uid

mole

fra

ctio

n

Column stage

Stearic acid

Methanol

SAME

Water

Figure 6: Liquid mole fraction profiles obtained from the optimization of the developed Aspen PLUS model.

In order to validate the values obtained from the optimization

carried out, the estimated optimum values of the operating

parameters were used to run the developed model of the plant

and the results obtained were as given in Figure 6 in terms of

the mole fraction profiles of the components present in the

column at steady state. The trends of the profiles of the

components obtained (Figure 6) were found to be similar to

those of the initial simulation carried out (Figure 2) except at

the bottom section. Also, in this case, an increment was

noticed to occur in the mole fraction of the desired product

present in the bottom product of the process collected from

the reboiler section.






4. Conclusion

The results obtained from the simulations of the reaction

integrated distillation process used for the production of

stearic acid methyl ester (SAME) carried out when the reflux

ratio was varied from 1 to 10 and the reboiler duty varied

from 0.1 to 1 kW revealed that high purity SAME could be

obtained at a reflux ratio of 1 and a reboiler duty of 0.1 kW,

separately, even though the combination of these values of

the operating parameters (reflux ratio and reboiler duty)

could not converge when used to run the developed model of

the process. Furthermore, using the optimum reflux ratio and

reboiler duty estimated to be 2.23 and 0.90 kW, respectively

to run the developed Aspen PLUS process model, SAME (a

biodiesel) mole fraction of 0.9993 was obtained from the

bottom product of the column. Therefore, it has been

discovered that each of reflux ratio and reboiler duty

separately affects the operation of the reaction integrated

distillation process, but in order to obtain high purity of

biodiesel, their combined effects should be simultaneously

studied and optimized.

5. Acknowledgement

Special thanks go to Aare Afe Babalola, LL.B, FFPA,

FNIALS, FCIArb, LL.D, SAN, OFR, CON. - Founder and

President, and the Management of Afe Babalola University,

Ado-Ekiti, Ekiti State, Nigeria for providing a very

conducive environment that enabled us to carry out this

research.

6. Nomenclature

Keq Equilibrium constant

RDBPROD Reaction integrated distillation bottom

product

RDCOLUMN Reaction integrated distillation column

RDLFEED Reaction integrated distillation lower feed

RDTPROD Reaction integrated distillation top product

RDUFEED Reaction integrated distillation upper feed

SAME Stearic acid methyl ester

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Author Profile

Dr. Abdulwahab GIWA was born in Ile-Ife, Osun

State, Nigeria in 1976. He obtained his National

Diploma in Chemical Engineering from Kaduna

Polytechnic, Kaduna, Nigeria in 1998 with a

Distinction Grade as the Best Student of the Programme.

Furthermore, he received his Bachelor Degree in Chemical

Engineering from Federal University of Technology, Minna,

Nigeria in 2004 with First Class Honours as the Best Student in

School of Engineering and Engineering Technology. Moreover, he

got his PhD Degree from Ankara University, Ankara, Turkey in

2012, also in the field of Chemical Engineering, with a Cumulative

Grade Point Average (CGPA) of 4.00 out of 4.00. Thereafter, he

proceeded to Middle East Technical University, Ankara, Turkey to

have his Postdoctoral research experience between 2012 and 2013.

He is currently a Senior Lecturer with the Department of Chemical

and Petroleum Engineering, Afe Babalola University, Ado-Ekiti,

Ekiti State, Nigeria. He is very interested in researches in the areas

of Process Modelling, Simulation, Optimization, Design and

Control.

Dr. (Mrs.) Saidat Olanipekun GIWA was born in

Oyo, Oyo State, Nigeria, in 1980. She received her

Bachelor Degree in Chemical Engineering from

Federal University of Technology, Minna, Nigeria in

2006 and her PhD Degree, also, in Chemical Engineering from

Ankara University, Ankara, Turkey in 2013. She is currently a

Lecturer in the Department of Chemical Engineering, Abubakar

Tafawa Balewa University, Bauchi, Nigeria. Her research interests

include Water Treatment Process Modelling, Simulation,

Optimization, and Control.


Documents

Investigating the Effects of Operating Parameters of a … · · 2017-07-22of reflux ratio and reboiler duty separately affects the operation of the reaction integrated distillation